Aluminum chlorhydroxy complex and borate gel



Patented July 14, 1 953 UNITED s r .TE Q

ALUMINUM onronnvnnoxr ooM LEX' I AND'BORATE GEL Thomas Govett, Summit, and Mildred' L. quist, Maplewood, N. .L, assigno'rsio Reheis Company, Inc., a. corporation of New York No Drawing.

' As described in thecopending application, there is -'used, as the-base material in making the gel,

a basic ohloridecontaining aluminum, chlorine, and hydroxyl groups in the ratio of 5-7 atoms of aluminum for 3 of chlorine and a sufficient numberof hydroxyl groups to make the total of the hydroxyl groups and chlorine atoms 3 for each atom of aluminum. A representative material of this type may be represented by the empirical formula A1sC13(OH) 15. Y

In our earlier application there is described also the use of borax or other borate to cause aqueous solutions of the selected aluminum chlorhydroxy complex to form a combination that gels in water Without the need of adding any organic emoluent or organic gelations material.

Gels somade are either too stifi at'low temperatures for some purpose or too soft at elevated temperatures. Additives that are effective for correcting one of these conditions should be expected to aggravate the other. The present invention provides a composition and method for extending the temperature range over which the gel may: be-used, as in a collapsible tube with an outlet for extrusion of the gel, so that thegel is neither toosoft at elevated summer temperatures nor. too stiff at normal winter room temperatures.

In. otherwords, the invention provides for decreasing the temperature susceptibility of the.

product or raising the temperature of objectionable softening above that previously possible without a corresponding increase in the stiffness at low temperatures.

Briefly stated, the invention comprises-the additionof an alcohol to the aqueous combination of boratev and aluminum vchlorhydroxy complex;

corporation also of a polyhydric alcohol such as glycerineserving as alubricant to increase the extrudability at low temperatures without. producing an obj ectionably low softening point:

As'to materials, the gel combinationto be modified is anyone. of those made with the-aluminum chlorhydroxyj complex and borax or other borate In. a modification, the invention comprises the .in-

ApplicationOctober 17, 1951, Serial No. 251,824

5 Claims. (01. 25 2 s17 2* as described in the said copending application, namely, gelscQntainingB-T atomic proportions of aluminum to 30f chlorine and a borate' as in the proportion corresponding to"1-5 atoms of boron for 9 of aluminum. From the gels of compositions within this range. we prefer for the present purpose those that are relatively very soluble in water. Examples are those in which the number of atoms of aluminum are 5-6 for 3 of chlorine,

11 the boron content remaining within the range stated previously.

To provide the borate content of the gel, there is used borax or other alkali metal salt of a bo-ric acid, examples being potassium tetraborate or 3 potassium, sodiumor amm'onium'orthoborate or metaborate. g

The alcohol used to decrease the temperature susceptibility or change of consistency of the gel with temperature is a monohydric aliphatic alcohol that is miscible in all proportions with water and that is non-toxic under conditions of use of the finished gel. Sincethe finished gel is useful as an astringent and as a base in cosmetic and. pharmaceutical preparations, methanol .is ordii narily avoided because of its toxicity. Alcohols that meet other general requirements statedand that are used satisfactorily are ethanol, isopropanol, and -3'butanol. v

"As the lubricant there is used a polyhydric alcohol that'is 'water's'oluble and non-toxic under the conditions of use" and is a liquidthat in the proportion useddoe's' notproduce water insolubility of the aluminum chlo'rhydroxy complexand I borate gel. In meeting these requirements, glyce'rine is outstanding. 'Since it is available ordinarily at a reasonable price, we use the glycerine as the lubricant to decrease-the stifiness of our gel at low temperatures The non-toxic, nonirritating glycols also meet the requirements'and may be used, as for example, propylenev and di-v ethylene jglycol. H

Water is used in addition to the special additives in the gel.

chlorhydroxy complex and'borate gelmay be used in lower concentration inthe improved gels than in those described in the-copending application, without loss of the desired consistency of the gel. Thus we find that a gel made as described herein, with the alcohol additive and with 7.05% of the aluminum clilorhydroxy and borate eL-calculated as aluminum oxide; is satisfactory in consistency at the temperatures of use or storage varying over a considerable range. 'A-similar gel Without the added alcohol, on the other hand, would require approXimately"l(i% :of fthe 'gel so, calculated for As to proportions, the aluminum- 9 of aluminum.

As to the liquid medium for the gel, the proportion of the monohydric alcohol is made to be approximately -30 parts for 100 parts of totalweight of the said chlorhydroxy complex, monohydric alcohol, and water. For most purposes we use -20 parts of the monohydric alcohol for 100 parts of it and water, all proportions, here and elsewhere herein being expressed as parts by weight except as indicated in the case" of the atomic proportions.

As the lubricant, glycerine is used in the proportion of approximately 2-10 parts for 100 of the total weight of the finished product. i

In compounding, the selected ingredients in the proportions stated are mixed suitably in warm condition. The alcohol or the mixture of alcohol and glycerine to be used may be incorporated with the water at the time the inorganicconstituents are dispersed in the water. Inan alternative procedure, the aluminum chlorhydroxy and borate compound are. first dissolved in. the water in hot condition and the alcohol or the alcohol and glycerine are then added and stirred into the hot solution. In case the temperature ofthe mix to which the alcohol is to be added is so high as would cause substantial loss of alcohol byboiling or evaporation, the solution is first cooled to below the boiling point of the alcohol before the alcohol is added; or in an alternative procedure, the alcohol is introduced in an autoclave which will necessarily restrict the evaporation of alcohol.

The invention will be illustrated in greater detail by description in connection with the following specific examples of the practice of it.

' The aluminum chlorhydroxy and borate gel, serving as the starting material for modification in the examples, was first prepared as vfollows: 200 parts of aluminum chlorhydroxy complex containing 6 Al to 301, equivalentto approxi-. mately 47% A1203, were dissolved in- 200 parts of water and the solution broughtto the temperature of 60 C. 40 parts of. borax were. dissolved separately in 449 parts of water and added with stirring to'the said solution at 60 C. .The resulting material (hereinafter referred to as Solution A") contains aluminum equivalent to 10.6% A1203 and, if it were cooled, would set to a gel of properties to be-improved by the additives shown in the specific examples that follow.

Example 1 A composition is made of the following 'formula:

The additives shown were stirred into the Solution A in warm condition at a temperature of 60 C. The product when cooled was a gel ready for use.

Example 2 The formula and procedure of. Examplev 1.: were 4 used except that propylene glycol was substituted on an equal weight basis for the glycerine.

Example 3 The procedure of Example 1 is used except that the formulawas as follows: I

Ingredient tg gfi Solution'A; 66. 7 Ethanol, approx 15 Glycerin; 3 Propylene glycol 3 Water l l2. 3

Total 100. 0

Example 4 The procedure and. formulas of any of the Examples 1 to 3 above are used except that isopropanol and 3-butano1 are substituted, in turn, for the ethanol on an equal weight basis;

Example 5'- The procedure and formula of any onev of. the Examples 1 to 4 above are used except thatthe aluminum chlorhydroxy and borax complex used (Solution A) is one made with the AlzCl ratio 5:3 or 7:3 and preferably 5:3.

I Example 6 In this example, the borax used in making the Solution A is replaced by any of the other borates listed earlier herein, all othermaterials, proportions, and conditions being as stated in the Examples 1 to 5. i v

Example 7' The procedure and formula of Example 1" are modified by replacement of the glycerine by an equal Weight of diethylene glycol. I

The products made'as described herein and particularly in the examples, set on cooling to a gel of low temperature susceptibility. The gel remains solid at temperatures up to F. but is soft enough to be extruded at normal winter indoor temperatures.

W Example 8 In a modification of the invention giving a stiffer, less extrudable' gel which is satisfactory its admixture with water, to form a liquid aqueous alcoholic dispersing medium, causes in the degree of dispersion of the gel forming particles and that glycerine and the like serve as internal lubricants, promoting flow of the particles of gel past and over each other, even at low temperatures.

It will be understood that it is intended to coverall changes and modifications of the examples of the invention herein chosen for the purpose of illustration which do not constitute departures from the spirit and scope of themvention.

What is claimed is:

1. A gel consisting essentially of the combination of aluminum chlorhydroxy complex and an' alkali metal borate; a water: solublenon-toxic:

been' aliphatic monohydric alcohol, and water, the ratios of aluminum, chlorine and boron being 5-? atomic proportions of aluminum to 3 of chlorine and 1-5 atomic proportions of boron to 9 of aluminum, and 100 parts by weight of the gel containing the monohydric alcohol in the proportion of 5-30 parts, the said combination of the complex and borate in amount to establish the desired consistency, and water in amount to make the total weight of the gel 100 parts.

2. The gel of claim 1 in which the monohydric alcohol is ethanol.

3. A gel consisting essentially of the combination of aluminum chlorhydroxy complex and an alkali metal borate, a water soluble non-toxic aliphatic monohydric alcohol, a water soluble non-toxic polyhydric alcohol serving as a lubricant in the gel, and water, the ratios of aluminum, chlorine, and boron being 5-7 atomic proportions of aluminum to 3 of chlorine and 1-5 atomic proportions of boron to 9 of aluminum, and 100 parts by weight of the gel containing 5-30 parts of the monohydric alcohol, 2-10 parts of the polyhydric alcohol, the said combination of complex and borate in amount to establish the desired consistency, and Water in amount to make the total weight of the gel 100 parts.

4. 'The gel of claim 3 in which the polyhydric alcohol is glycerine.

5. The gel of claim 3 in which the polyhydric alcohol is a glycol.

' THOMAS GOVETT.

MILDRED L. ALMQUIST.

No references cited. 

1. A GEL CONSISTING ESSENTIALLY OF THE COMBINATION OF ALUMINUM CHLORHYDROXY COMPLEX AND AN ALKALI METAL BORATE, A WATER SOLUBLE NON-TOXIC ALIPHATIC MONONHYDRIC ALCOHOL, AND WATER, THE RATIOS OF ALUMINUM, CHLORINE AND BORON BEING 5-7 ATOMIC PROPORTIONS OF ALUMINUM TO 3 OF CHLORINE AND 1-5 ATOMIC PROPORTIONS OF BORON TO 9 OF ALUMINUM, AND 100 PARTS BY WEIGHT OF THE GEL CONTAINING THE MONOHYDRIC ALCOHOL IN THE PROPORTION OF 5-30 PARTS, THE SAID COMBINATION OF THE COMPLEX AND BORATE IN AMOUNT TO ESTABLISH THE DESIRED CONSISTENCY, AND WATER IN AMOUNT TO MAKE THE TOTAL WEIGHT OF THE GEL 100 PARTS. 